CN1390775A - Microwaye excited transfer process for preparing hydrogen from methane - Google Patents
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Abstract
A microwave exciting process for preparing hydrogen from methane features that the raw methane is stayed in reaction region for 1-10 seconds, the substance which easily discharges under the excitation of electromagnetic field is arranged in the reaction region, and the reaction region is radiated by continuous or pulse microwaves to make said substance discharge, which can generate plasma to crack methane, so obtaining hydrogen. Its advantages are high transform rate of methane, easy control, high safety and high purity of hydrogen.
Description
The present invention relates to the methane conversion hydrogen producing technology, microwave excitation methane conversion process for making hydrogen is provided especially.
Hydrogen is important chemical goods and materials and energy and material.Especially under the environment requirement of preserving our planet, hydrogen gets most of the attention as the fuel that cleans most.The main energy sources material of our times is a fossil oil, and the burning of fossil oil will produce a large amount of carbonic acid gas, and obnoxious flavoures such as carbon monoxide, the Greenhouse effect of the earth just use closely related with a large amount of burnings of fossil oil.And the product of hydrogen burning has only water, and is nuisanceless pollution-free.But natural hydrogen resource seldom, and it mainly obtains by decomposing other hydrogen-containing compound.Methane is the major ingredient of Sweet natural gas, and the reserves of Sweet natural gas are very abundant on the earth, and the exploration result shows that the total resources of Sweet natural gas is also more than the summation of coal and oil.Methane is elementary composition by carbon and two kinds of hydrogen, and its cracking can produce hydrogen.Therefore preparing hydrogen from resourceful methane has better industrial application prospect.Existing approach from methane hydrogen manufacturing mainly contains to sow:
1, partial oxidation of methane hydrogen.The principal feature of this technological process has: the methane conversion height,
The selectivity height of hydrogen, the reaction velocity height.But this reaction process is at high temperature carried out, and needs
Want the oxygen feeding of high density, the reaction process complexity, the reaction process security is lower, and
And hydrogen, carbon monoxide concentration that this process produces are higher, have certain office on using
Sex-limited.[Production?of?synthesis?gas，Catal.Today?18(1993)305-324]
2, the hydrogen manufacturing of methane steam reforming.The principal feature of this technological process is: the methane conversion height,
The selectivity height of hydrogen, reaction process is safer.But this reaction process needs high temperature and big
Water gaging steam, reaction process energy consumption height, complex process, carbon monoxide concentration in the product hydrogen
Height, range of application is restricted.[Production?of?synthesis?gas，Catal.Today
18(1993)305-324]
3, the principal feature of this technological process of arc process cracking methane hydrogen manufacturing is: the methane conversion height,
Technology is simple, and product hydrogen does not contain carbon monoxide, applied range.But reaction process is not
Easy to control, energy consumption is too high, can only be used for the flourishing area of water power.[from coal and Sweet natural gas
Produce acetylene and derivative thereof, Chemical Industry Press (1992)]
4, under the microwave exposure there be the principal feature of this technological process of methane hydrogen manufacturing: the methane conversion height,
Reaction process is controlled easily, and is safe, and product hydrogen does not contain carbon monoxide, range of application
Extensively.But this reaction needed is carried out under negative pressure, is unfavorable for large-scale industrial production,
Thereby be in the research.[U.S. Pat 4574038, Decomposition of
hydrocarbons?in?a?microwave?discharge，J.Phys.Chem.，Volume
73，number?6，6(1969)]
In order to overcome the problems referred to above, the technology that the purpose of this invention is to provide the hydrogen manufacturing of a kind of microwave excitation methane conversion, it is that the gas that contains finite concentration methane under the certain pressure passes through reaction zone with certain flow rate, be placed with the object that easily discharges under the electromagnetic field effect in the reaction zone, use then continuously or pulse microwave carries out radiation to reaction zone, the material that electromagnetic field effect easily discharges is down transferred the electroinitiation plasma body at microwave action, thereby cracking methane is produced hydrogen.The characteristics of this process are the methane conversion height, and reaction process is controlled easily, and are safe, and technology is simple, and product hydrogen does not contain carbon monoxide, applied range, and reaction can be carried out at normal pressure or more than the normal pressure, can large-scale industrial production.
Specifically, the technology of a kind of microwave excitation methane conversion provided by the invention hydrogen manufacturing, be to make methane gas pass through reaction zone, be placed with the material that easily discharges under the electromagnetic field effect in the reaction zone, use microwave that reaction zone is carried out radiation then, the material that electromagnetic field effect easily discharges is down transferred the electroinitiation plasma body at microwave action, thereby cracking methane is produced hydrogen, it is characterized in that, methane-containing gas pressure is 1-3 standard atmospheric pressure in the reaction zone, and the frequency of microwave should be greater than 0.3GHz, and the power input minimum is 5W.
In above-mentioned the present invention, the material that the electromagnetic field effect of placing in the reaction zone easily discharges down can be platinum, tungsten, iron, nickel, copper and their alloy or mixture, and best optional tungsten is as discharging substance.
In addition, in above-mentioned the present invention, the material that the electromagnetic field effect of placing in the reaction zone easily discharges down also can be graphite, gac, silicon carbide, wolfram varbide, molybdenum carbide and composition thereof, and is preferably graphite.
In addition, in above-mentioned the present invention, concentration of methane gas is the 1%-100% volumn concentration, is applicable to a large amount of methane-containing gas kinds, as catalytic cracked dry gas, and Sweet natural gas, coal-seam gas etc.And preferably concentration of methane gas is chosen as 50%-100%.
In above-mentioned the present invention, methane-containing gas is 1-10 second in the reaction zone residence time, and the residence time, long more methane conversion was high more, and density of hydrogen is high more in the tail gas.But surpass 10 seconds when the residence time, methane conversion is almost 100%, and density of hydrogen also is difficult to improve again in the tail gas, and overstand influences the productive rate of product, is unfavorable for suitability for industrialized production.Therefore, the residence time preferably is no more than 10 seconds.
In addition, in above-mentioned the present invention, the microwave that acts on reaction zone can be continuously or pulsed, is applicable to most of existing microwave devices.As long as and its microwave frequency can reach 0.3GHz, power input surpasses 5W just can carry out conversion of methane.But, act on usually reaction zone continuously or the frequency of pulse microwave be 0.915,2.45,5.80 or 22.0GHz, power input is more than the 100W, and improves power input and help methane conversion Cheng Qing.Concrete power input can be set according to real reaction requirement and condition.
In addition, in above-mentioned the present invention, the duty that acts on the pulse microwave of reaction zone can be 0.1-1, and pulse-repetition can be 1-10Hz.
In the present invention, the primary product of methane conversion is hydrogen and carbon, by-product a little acetylene, ethene.
Compare the present invention with known technology and have following distinguishing feature:
1. reactant gases is at normal temperature and normal pressure or can be initiated more than the normal pressure and react, and the activation temperature of methane need be higher than 1200 ℃ under the catalyst-free condition, and plasma-converted methane needs condition of negative pressure under the normal temperature at normal pressure usually.High temperature and negative pressure are the two big difficulties of methane activation process on industrialization road.The present invention is by placing the easily object of discharge in reaction zone, under continuous or pulse microwave effect, cause this process of discharge plasma and realize methane conversion, methane can be initiated at normal temperatures to react, can guarantee to be reflected at normal pressure again or be higher than stable carrying out under the normal pressure, this will help the process of industrialization of Sweet natural gas comprehensive utilization undoubtedly.
2. among the present invention, the conversion process of methane need not to use catalyzer, has avoided many difficulties that often run in catalyzed reaction, and this has simplified technical process undoubtedly greatly, has reduced the conversion cost of methane, more helps the further application of this process.
3. among the present invention, tail gas hydrogen concentration height does not contain carbon monoxide in the product hydrogen, and range of application is very extensive, is particularly useful for the proton membrane fuel battery field to carbon monoxide poisoning.
4. among the present invention, use microwave as energy derive, clean and safe, and also the response of microwave energy supplying system is rapidly, and production process is controlled easily, and is safe.
State the present invention below by embodiment is auspicious:
Embodiment 1. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters metal bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the reaction gas that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply the continuous microwave radiation, power 100W, frequency 2450MHz regulates short-circuit plunger, makes microwave reflection power reach minimum, the metal bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.The results are shown in table 1:
Table 1 different metal discharging substance is to the influence of reaction result
| Discharging substance | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| Tungsten | ????96.1 | ????10.0 | ????1.0 | ????0 | ????89.0 | ????91.1 |
| Platinum | ????95.8 | ????11.1 | ????1.2 | ????0 | ????88.7 | ????90.2 |
| Iron-nickel alloy | ????96.5 | ????9.5 | ????0.8 | ????0 | ????89.7 | ????92.2 |
Embodiment 2. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters carbon or carbide rod vertically place on the reaction tubes axis and are positioned at microwave resonator central authorities, the reaction gas that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply the continuous microwave radiation, power 100W, frequency 2450MHz regulates short-circuit plunger, makes microwave reflection power reach minimum, carbon or carbide rod tip produce discharge with this understanding and cause plasma body, thereby the methane cracking produces hydrogen.The results are shown in table 2:
Different carbon of table 2 or carbide discharging substance are to the influence of reaction result
| Discharging substance | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| Silicon carbide | ????96.0 | ????11.1 | ????1.2 | ????0 | ????87.8 | ????89.1 |
| Graphite | ????96.1 | ????10.8 | ????1.1 | ????0 | ????88.1 | ????90.2 |
Embodiment 3. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the gas of different methane concentrations is fed reaction tubes, the diluent gas of reaction gas is an argon gas, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply the continuous microwave radiation, power 100W, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.The results are shown in table 3.By table 3 result as can be known, improve methane concentration and make density of hydrogen increase in the product.And it is little for selectivity of product influence beyond the dehydrogenation.
The different methane concentrations of table 3 are to the influence of reaction result
| Methane concentration/mol% | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ????1 | ????99.3 | ????10.3 | ????1.5 | ????0 | ????88.2 | ????0.9 |
| ????50 | ????99.0 | ????10.1 | ????1.1 | ????0 | ????88.8 | ????49.1 |
| ????100 | ????96.1 | ????10.0 | ????1.0 | ????0 | ????89.0 | ????91.1 |
Embodiment 4. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the reactant gases that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, apply the continuous microwave radiation, power 100W, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.Reaction gas pressure not simultaneously, different reaction results are listed in table 4.By table 4 result as can be known, the processing method of methane conversion hydrogen manufacturing of the present invention can or add at normal pressure to depress and carries out.Help large-scale industrialization production like this.
Table 4 differential responses pressure is to the influence of reaction result
| Pressure/atm | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ????1 | ????96.1 | ????10.0 | ????1.0 | ????0 | ????89.0 | ????91.1 |
| ????2 | ????97.2 | ????9.0 | ????0.8 | ????0 | ????90.2 | ????92.2 |
| ????3 | ????98.0 | ????8.0 | ????0.7 | ????0 | ????91.3 | ????93.2 |
Embodiment 5. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the gas that will contain methane 100% feeds reaction tubes, reaction gas pressure is 1 standard atmospheric pressure, apply the continuous microwave radiation, power 100W, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.The reaction result difference the results are shown in table 5 to reactant gases not simultaneously the residence time in microwave resonator.By table 5 result as can be known, methane is long more in the reaction zone residence time, and the concentration of hydrogen is high more in the product.
The different residence time of table 5 are to the influence of reaction result
| The residence time/second | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ????1 | ????84.0 | ????77.5 | ????2.1 | ????0.4 | ????20.0 | ????81.8 |
| ????5 | ????96.1 | ????10.0 | ????1.0 | ????0 | ????89.0 | ????91.1 |
| ????10 | ????99.0 | ????2.7 | ????0.3 | ????0 | ????97.0 | ????97.2 |
Embodiment 6. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the gas that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply the continuous microwave radiation, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.Microwave input power not simultaneously, the reaction result difference the results are shown in table 6.As shown in Table 6, the microwave power raising being helped methane conversion is hydrogen.
The different microwave input power of table 6 are to the influence of reaction result
| Microwave power/W | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ??5 | ????15.0 | ????76.0 | ????2.2 | ????0 | ????21.8 | ????11.0 |
| ??5 | ????70.8 | ????35.2 | ????1.8 | ????0 | ????63.0 | ????80.9 |
| ??100 | ????96.1 | ????10.0 | ????1.0 | ????0 | ????89.0 | ????91.0 |
| ??500 | ????98.0 | ????8.0 | ????0.6 | ????0 | ????91.4 | ????93.2 |
Embodiment 7. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the gas that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply pulsed microwave radiation, dutycycle is 0.1, power 100W, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.The microwave pulse frequency not simultaneously, the reaction result difference the results are shown in table 7.As shown in Table 7, improve pulse-repetition, help improving density of hydrogen.The different microwave pulse frequencies of table 7 are to the influence of reaction result
| Pulse-repetition/Hz | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ????1 | ????66.0 | ????53.2 | ????2.7 | ????0 | ????44.1 | ????78.2 |
| ????5 | ????80.0 | ????35.0 | ????2.1 | ????0 | ????62.9 | ????85.0 |
| ????10 | ????85.2 | ????28.0 | ????1.8 | ????0 | ????70.2 | ????87.6 |
Embodiment 8. is that 25 millimeters crystal reaction tube places microwave resonator with internal diameter, with one section diameter is 3 millimeters, long 10 millimeters tungsten bar vertically places on the reaction tubes axis and is positioned at microwave resonator central authorities, the gas that will contain methane 100% feeds reaction tubes, reactant gases residence time in microwave resonator is 5 seconds, reaction gas pressure is 1 standard atmospheric pressure, apply pulsed microwave radiation, pulse-repetition 5Hz, power 100W, frequency 2450MHz, regulate short-circuit plunger, make microwave reflection power reach minimum, the tungsten bar tip produces discharge with this understanding and causes plasma body, thereby the methane cracking produces hydrogen.The pulse microwave dutycycle not simultaneously, the reaction result difference the results are shown in table 8.As shown in Table 8, improve the pulse microwave dutycycle and help methane conversion, and can improve the selectivity of hydrogen.
The different microwave pulse dutycycles of table 8 are to the influence of reaction result
| Dutycycle | Methane conversion/% | Selectivity of product/% beyond the dehydrogenation | Density of hydrogen/mol% | |||
| Acetylene | Ethene | Ethane | Carbon | |||
| ??0.1 | ????70.0 | ????51.0 | ????2.5 | ????0 | ????46.5 | ????80.2 |
| ??0.5 | ????80.0 | ????35.0 | ????2.1 | ????0 | ????62.9 | ????85.0 |
| ??1 | ????90.6 | ????22.0 | ????1.5 | ????0 | ????76.5 | ????89.8 |
Claims (9)
1. the technology of microwave excitation methane conversion hydrogen manufacturing, be to make methane gas pass through reaction zone, be placed with the material that easily discharges under the electromagnetic field effect in the reaction zone, use microwave that reaction zone is carried out radiation then, the material that electromagnetic field effect easily discharges is down transferred the electroinitiation plasma body at microwave action, thereby cracking methane is produced hydrogen, it is characterized in that, methane-containing gas pressure is 1-3 standard atmospheric pressure in the reaction zone, and the frequency of microwave should be greater than 0.3GHz, and the power input minimum is 5W.
2. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that the electromagnetic field effect of placing in the reaction zone material of easy discharge down is platinum, tungsten, iron, nickel, copper and their alloy or mixture.
3. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that the electromagnetic field effect of placing in the reaction zone material of easy discharge down is graphite, gac, silicon carbide, wolfram varbide, molybdenum carbide and composition thereof.
4. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that concentration of methane gas is the 1%-100% volumn concentration.
5. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that concentration of methane gas is the 50%-100% volumn concentration.
6. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that methane-containing gas is 1-10 second in the reaction zone residence time.
7. by the technology of the described microwave excitation methane conversion of claim 1 hydrogen manufacturing, it is characterized in that the microwave that acts on reaction zone can be continuously or pulsed.
8. by the technology of the described microwave excitation methane conversion of claim 6 hydrogen manufacturing, it is characterized in that, act on reaction zone continuously or the frequency of pulse microwave be 0.915,2.45,5.80 or 22.0GHz.
9. by the technology of the described microwave excitation methane conversion of claim 6 hydrogen manufacturing, it is characterized in that the dutycycle that acts on the pulse microwave of reaction zone is 0.1-1, pulse-repetition is 1-10Hz.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944238B (en) * | 2006-10-16 | 2010-05-12 | 鲍涛 | Process for preparing high purity hydrogen and carbon black by microwave mediation |
| CN103011076A (en) * | 2011-11-03 | 2013-04-03 | 吉林大学 | Vehicle-mounted microwave low-temperature plasma reformer system for online hydrogen production |
| CN106185806A (en) * | 2016-07-01 | 2016-12-07 | 中国科学院电工研究所 | A kind of device and method utilizing plasma-converted methane |
| CN110201617A (en) * | 2019-07-03 | 2019-09-06 | 西安交通大学 | A kind of high energy reaction starting method |
| CN111411001A (en) * | 2020-04-20 | 2020-07-14 | 广东石油化工学院 | Device and method for promoting methane conversion |
| CN114408899A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of nano high-purity carbon |
| CN115259983A (en) * | 2022-08-22 | 2022-11-01 | 大连理工大学 | Method for preparing ethylene by anaerobic coupling of methane |
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- 2001-06-07 CN CNB011187212A patent/CN1180976C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944238B (en) * | 2006-10-16 | 2010-05-12 | 鲍涛 | Process for preparing high purity hydrogen and carbon black by microwave mediation |
| CN103011076A (en) * | 2011-11-03 | 2013-04-03 | 吉林大学 | Vehicle-mounted microwave low-temperature plasma reformer system for online hydrogen production |
| CN103011076B (en) * | 2011-11-03 | 2014-07-16 | 吉林大学 | Vehicle-mounted microwave low-temperature plasma reformer system for online hydrogen production |
| CN106185806A (en) * | 2016-07-01 | 2016-12-07 | 中国科学院电工研究所 | A kind of device and method utilizing plasma-converted methane |
| CN106185806B (en) * | 2016-07-01 | 2018-07-31 | 中国科学院电工研究所 | A kind of device and method using plasma-converted methane |
| CN110201617A (en) * | 2019-07-03 | 2019-09-06 | 西安交通大学 | A kind of high energy reaction starting method |
| CN111411001A (en) * | 2020-04-20 | 2020-07-14 | 广东石油化工学院 | Device and method for promoting methane conversion |
| CN114408899A (en) * | 2022-01-26 | 2022-04-29 | 株洲科能新材料股份有限公司 | Preparation method of nano high-purity carbon |
| CN115259983A (en) * | 2022-08-22 | 2022-11-01 | 大连理工大学 | Method for preparing ethylene by anaerobic coupling of methane |
| CN115259983B (en) * | 2022-08-22 | 2023-11-10 | 大连理工大学 | Method for preparing ethylene by methane anaerobic coupling |
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